| 杨华剑,胡晓燕,何计龙.SPE-氢化物发生原子荧光联用技术测定昆布中的无机砷含量[J].中国海洋药物,2016,35(4):71-75. |
| SPE-氢化物发生原子荧光联用技术测定昆布中的无机砷含量 |
| Determination of inorganic arsenic in kelp by SPE HG-AFS |
| 投稿时间：2016-03-16 修订日期：2016-04-19 |
| DOI： |
| 中文关键词: 昆布 原子荧光 固相萃取 无机砷 |
| English Keywords:Kelp, Atomic fluorescence spectrum(AFS), SPE, inorganic arsenic |
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| 中文摘要: |
| 目的： 建立氢化物发生原子荧光测定昆布中无机砷含量(As ( III)和As (V))的方法。方法：采用1%硝酸90℃水浴提取昆布中的无机砷,5%双氧水氧化As ( III)成As (V)。以强阴离子交换SPE技术消除MMA、DMA的干扰,无机砷以As (V)形式洗脱。氢化物发生原子荧光法测定无机砷。结果：线性范围为0-20mg/L,线性相关系数0.9997,加样回收试验低、中、高浓度平均回收率分别为83%、90%、92%,样品7次测定RSD为5.3%,方法检出限0.046mg/L。测定结果与HPLC-ICP-MS法结果比对满意。结论：本方法操作简便,仪器配置要求低,满足分析测试要求,适用于一般实验室昆布中无机砷的测定。 |
| English Summary: |
| Objective: To establish a method for the determination of inorganic arsenic (As ( III) and As (V))in kelp by hydride generation atomic fluorescence spectrum(HG-AFS). Methods: Inorganic arsenic was extracted by 90℃ water bath with 1% HNO3. As ( III) was oxidised by 5% H2O2. MMA、DMA were removed using strong anion exchange solid phase extraction(SPE). The inorganic arsenic was eluated from the SPE as As (V)). Then the inorganic arsenic was detected by HG-AFS. Results: The linearity of this method ranged from 0 to 20mg/L and the correlation coefficient was 0.9997. The limit of detection was 0.046mg/L. The average spiked recoveries were 83%, 90%, 92% at low, medium and high concentrations, respectively. RSD of the repeatability was 5.6%. Conclusion: This method is accurate, simple, feasible and rapid. It could be used for the determination of inorganic arsenic in kelp. |
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